JP6600023B2 - 優れた密着力を有する銅箔、それを含む電極、それを含む二次電池、およびその製造方法 - Google Patents
優れた密着力を有する銅箔、それを含む電極、それを含む二次電池、およびその製造方法 Download PDFInfo
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Description
延伸強度率(kgf/mm2)=降伏強度(kgf/mm2)×延伸率値
ここで、延伸率値は単位がない。
酸素含量はオージェ電子分光法(Auger Electron Spectroscopy:AES)により測定され得る。
・電子エネルギー分析器(Electron Energy Analyzer):CMA(Cylindrical Mirror Analyzer)
・電子ビームエネルギー(Electron Beam Energy):5 KeV
・ターゲット電流(Target Current):10nA
・チルト(Tilt):30degrees
・アルゴン食刻率(Etching Rate):SiO2基準60A/min(3KVのアルゴンイオンビーム)
延伸強度率(kgf/mm2)=降伏強度(kgf/mm2)×延伸率値
式1において、延伸率値は単位がない値である。
電解槽10、電解槽10に配置された回転陰極ドラム12および回転陰極ドラム12と所定間隔離隔した正極板13を含む製箔機を利用して銅箔を製造した。電解液11は硫酸銅溶液であり、硫酸銅溶液の銅イオンの濃度は75g/L、硫酸の濃度は100g/Lであり、硫酸銅溶液の温度は55℃に維持された。
JIS B 0601−2001規格に沿って粗さ計(Mitutoyo SJ−310モデル)を用いて銅箔の表面の最大高さ粗さ(Rmax)を測定した。この時、カットオフ(Cut off)の長さを除いた測定長さは4mm、カットオフ(Cut off)の長さは初期と末期をそれぞれ0.8mmにした。また、スタイラスチップ(Stylus Tip)の半径(Radius)は2μmにして、測定圧力は0.75mNにした。以上のように設定した後に測定してMitutoyo粗さ計の測定値基準で最大高さ粗さ(Rmax)値を得た。
ASME B46.1規格に沿って得られた表面粗さプロファイルで4mmの単位サンプリングの長さ当たり0.5μmの上位基準線上にそびえている有効ピークの個数を確認してピーク密度(PD)を測定した。
万能試験機(UTM)を利用してIPC−TM−650 Test Method Manualに規定した方法に沿って延伸率と降伏強度を測定する。延伸率と降伏強度測定用サンプルの幅は12.7mmであり、グリップ(Grip)間の距離は50mmであり、測定速度は50mm/minである。
延伸強度率(kgf/mm2)=降伏強度(kgf/mm2)×延伸率値
式1において、延伸率値は単位がない値である。
銅箔を切断して2cm×2cmの測定用サンプルを製造し、オージェ電子分光法(Auger Electron Spectroscopy:AES)用機器であるPHI700(ULVAC−PHI、INC.)を利用してサンプル第1面S1の原子の個数を測定した。分析条件は次のとおりである。
−電子エネルギー分析器(Electron Energy Analyzer):CMA(Cylindrical Mirror Analyzer)
−電子ビームエネルギー(Electron Beam Energy):5 KeV
−ターゲット電流(Target Current):10nA
−チルト(Tilt):30degrees
−アルゴン食刻率(Etching Rate):SiO2基準60A/min(3KVのアルゴンイオンビーム)
1)負極の製造
1−1)負極活物質の製造
負極活物質として人造黒鉛およびSiO2混合物(95%:5%)、バインダーとしてスチレン−ブタジエンゴムおよび増粘剤でカルボキシメチルセルロースを97:1.5:1.5の重量比で混合した後、水に分散させて負極活物質用スラリーを製造した。
製造例1−6および比較例1−6で製造された銅箔を表面がきれいなガラス板の上に載置した後、シワ、カールが発生しないように広げておき、バーコーター(Bar coater)を利用して銅箔上に負極活物質用スラリーをコーティングした。負極活物質用スラリーのコーティング量は9.0±0.5mg/cm2であった。この時、バーコーター(Bar coater)の速度は10〜15mm/sであった。
負極活物質用スラリーがコーティングされた後、乾燥した銅箔試料をロールプレス(Roll press)を用いて圧着して電極を製造した。この時、電極密度が1.55±0.05g/ccとなるように4段圧着した。このような圧着によって銅箔に付着した負極活物質を含む電極が完成された。
2−1)密着力測定用試料製作
密着力を測定しようとする電極を、幅10mm×長さ100mmに切断した。
切断した電極の負極活物質の部分と補強板を両面テープで付着した。この時、製作されるすべての試料は均一な力で付着され得るようにした。
IPC−TM−650規格に沿って万能試験機(UTM)を利用して銅箔と負極活物質層の剥離強度を測定した。測定用サンプルの幅は12.7mmであり、測定速度は50mm/分であった。この時、90°剥離力が測定される(90°Peelingテスト)。すなわち、補強板と負極活物質層を両面テープで付着させて銅箔を90°に剥離しながら剥離強度を測定することによって、密着力を測定した。
(1)銅層110の形成過程での電流密度が80ADSを超過する比較例1および40ADS未満の比較例2;
(2)電解液内の全無機炭素量(TIC)が0.05g/Lを超過する比較例3;
(3)電解液内の鉄(Fe)イオンの濃度が0.30g/Lを超過する比較例4;
(4)防錆液のpHが1.5未満の比較例5および4.2を超過する比較例6;
(5)防錆液の溶存酸素量が5ppm以上である比較例6;
(6)最大高さ粗さ(Rmax)が0.6μm未満である比較例1および3.5μmを超過する比較例2;
(7)ピーク密度(PD)が5個未満の比較例3および110を超過する比較例4;
(8)延伸強度率が0.55未満の比較例1;および
(9)銅箔の表面の酸素含量が22at%未満である比較例5および67at%を超過する比較例6.
210、220:保護層
310:活物質層
300、400:二次電池用電極
340:二次電池用負極
370:二次電池用正極
MS:マット面
SS:シャイニー面
Claims (15)
- 銅層;および
前記銅層上に配置された保護層;
前記保護層の表面は0.6μm〜3.5μmの最大高さ粗さ(Rmax)、5個〜110個のピーク密度(Peak Density:PD)および22at%(atomic%、原子%)〜67at%の酸素含量を有する、銅箔。 - 前記保護層は、クロム、シラン化合物および窒素化合物のうち少なくとも一つを含む、請求項1に記載の銅箔。
- 25±15℃の常温で25kgf/mm2以上の降伏強度を有する、請求項1に記載の銅箔。
- 25±15℃の常温で2%以上の延伸率を有する、請求項1に記載の銅箔。
- 下記の式1で表現される、0.55kgf/mm2以上の延伸強度率を有する、請求項1に記載の銅箔:
[式1]
延伸強度率(kgf/mm2)=降伏強度(kgf/mm2)×延伸率値
ここで、延伸率値は単位がない。 - 4μm〜30μmの厚さを有する、請求項1に記載の銅箔。
- 銅箔;および
前記銅箔上に配置された活物質層;を含み、
前記銅箔は、
銅層;および
前記銅層と前記活物質層との間に配置された保護層;を含み、
前記銅箔の表面は0.6μm〜3.5μmの高さ最大粗さ(Rmax)、5個〜110個のピーク密度(PD)および22at%〜67at%の酸素含量を有する、二次電池用電極。 - 前記保護層は、クロム、シラン化合物および窒素化合物のうち少なくとも一つを含む、請求項7に記載の二次電池用電極。
- 前記銅箔は、25±15℃の常温で25kgf/mm2以上の降伏強度および2%以上の延伸率を有する、請求項7に記載の二次電池用電極。
- 正極(cathode);
請求項7〜請求項9のいずれか一項に記載された二次電池用電極からなる負極(anode);
前記正極と前記負極との間に配置されてリチウムイオンが移動できる環境を提供する電解質(electrolyte);および
前記正極と前記負極とを電気的に絶縁させる分離膜(separator);
を含む、二次電池。 - 銅イオンを含む電解液内に、互いに離隔するように配置された正極板および回転陰極ドラムを、40〜80A/dm2の電流密度で通電させて銅層を形成する段階;および
クロム(Cr)を含む防錆液内に前記銅層を浸漬させて、前記銅層上に保護層を形成させる段階;を含み、
前記防錆液は1.5〜4.2のpHおよび5ppm未満の溶存酸素量を有する、
銅箔の製造方法。 - 前記電解液は、70〜90g/Lの銅イオンおよび80〜120g/Lの硫酸を含む、請求項11に記載の銅箔の製造方法。
- 前記電解液内の全無機炭素量(Total Inorganic Carbon、TIC)は0.05g/L以下である、請求項11に記載の銅箔の製造方法。
- 前記電解液内の鉄(Fe)イオンの濃度は、0.30g/L以下である、請求項11に記載の銅箔の製造方法。
- 前記銅層の形成段階は、活性炭を利用して前記電解液を濾過する段階を含む、請求項11に記載の銅箔の製造方法。
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